CN114836057A - Preparation method of nano hydrated silicon dioxide super-hydrophobic modification - Google Patents
Preparation method of nano hydrated silicon dioxide super-hydrophobic modification Download PDFInfo
- Publication number
- CN114836057A CN114836057A CN202210365109.XA CN202210365109A CN114836057A CN 114836057 A CN114836057 A CN 114836057A CN 202210365109 A CN202210365109 A CN 202210365109A CN 114836057 A CN114836057 A CN 114836057A
- Authority
- CN
- China
- Prior art keywords
- silicon dioxide
- reaction kettle
- nano hydrated
- pressure
- hydrated silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of white carbon black modification methods, in particular to a method for preparing nano hydrated silicon dioxide by super-hydrophobic modification, through the combination of more than two kinds of preferable silane coupling agents and the gas-solid reaction of the nano hydrated silicon dioxide, the internal hydroxyl of the nano hydrated silicon dioxide is eliminated and is converted into lipophilicity, the application and the field of the method are expanded and deepened in the aspects of manufacturing high-temperature resistant oily paint and environment-friendly waste oil absorption products, and in the invention, after the modification reaction is finished, firstly, the reaction kettle is decompressed for one time to remove most of ammonia gas, then the decompression valve is closed, the nitrogen is introduced into the reaction kettle, so that the reaction kettle is pressurized again, the nitrogen fills the pores, and the residual ammonia is thoroughly removed by secondary pressure relief and vacuum pumping, thereby achieving the purpose of preparing the super-hydrophobic nano hydrated silicon dioxide product and not influencing the acid-base balance of a using system.
Description
Technical Field
The invention relates to the technical field of white carbon black modification methods, and particularly relates to a nano hydrated silicon dioxide super-hydrophobic modification preparation method.
Background
The nanometer hydrated silica is also called nanometer white carbon black, and is widely applied to the fields of rubber reinforcing agents, ink thickening agents, spraying materials, flatting agents and the like, and the nanometer hydrated silica has a large amount of active hydroxyl groups, has hydrophilicity and poor compatibility with organic matters, so that the application range of the nanometer hydrated silica is limited. When the method is applied to the fields of room temperature vulcanized silicone rubber, printing ink, paint, coating, adhesive, high-efficiency heat insulation materials, defoaming agents and dry powder extinguishing agents, most of the fields need to be subjected to hydrophobic treatment. At present, various production methods for hydrophobic modification of nano hydrated silicon dioxide are available, a single assistant treatment process is mostly adopted, the treatment agent dosage is large, the time is long, the energy consumption is high, the efficiency is low, and a super-hydrophobic product with the methanol value of more than 70 is difficult to prepare. Meanwhile, because a large number of pores exist among the nano hydrated silicon dioxide particles, the nano hydrated silicon dioxide has strong adsorbability, and a byproduct of modification reaction is easy to remain in the pores and is difficult to completely remove, so that the pH value of the prepared hydrophobic silicon dioxide is influenced when the hydrophobic silicon dioxide is used in an organic phase of a polysiloxane system, and the acid-base balance of the organic phase is influenced by partial acid or partial alkali, even the polysiloxane is subjected to condensation polymerization or decomposition. The product performance of the product is seriously influenced.
Therefore, how to improve the hydrophobic modification process of the nano hydrated silica, improve the hydrophobic treatment efficiency, remove the by-products generated during the treatment to the maximum extent, and develop the super-hydrophobic nano hydrated silica with high efficiency, energy conservation and neutral pH value becomes a technical problem which needs to be solved urgently.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to improve the hydrophobic modification process of the nano hydrated silicon dioxide, effectively improve the hydrophobic treatment efficiency, and simultaneously remove the by-product generated by the reaction to the maximum extent, so that the methanol value of the prepared super-hydrophobic nano hydrated silicon dioxide is more than 70, and the pH value is kept neutral.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for preparing nano hydrated silicon dioxide by super-hydrophobic modification comprises the following steps:
step 1: adding a silane coupling agent into a hydrolysate which is prepared by compounding organic acid, water and polyalcohol in advance for hydrolysis, wherein the silane coupling agent is prepared by compounding hexamethyldisilazane and one or more than two of A-171, A-151 and KH560 to obtain a coupling agent hydrolysate, and the coupling agent hydrolysate needs to be used up within 1 hour;
step 2: adding the nano hydrated silicon dioxide into a reaction kettle, sealing the reaction kettle, starting stirring and heating;
And 3, step 3: after the temperature of the material is raised to 100-110 ℃, spraying the hydrolyzed coupling agent solution into a reaction kettle in a fogging manner, raising the temperature of the material to 120-140 ℃, and carrying out a closed reaction for 30-50 min;
and 4, step 4: after the reaction is finished, opening a pressure release valve of the reaction kettle for pressure release, and then closing the pressure release valve; introducing high-pressure nitrogen into the closed reaction kettle, raising the pressure in the reaction kettle again to 3-4 MPa, maintaining for 30-50 min, and then slowly releasing the pressure;
and 5: and (3) after the pressure is relieved to normal pressure, carrying out negative pressure air extraction on the reaction kettle for 10-20 min, wherein the negative pressure is-0.03 MPa to-0.01 MPa, and finally obtaining the super-hydrophobic modified nano hydrated silicon dioxide product.
Further, in the method for preparing the nano hydrated silicon dioxide through super-hydrophobic modification, the organic acid is acetic acid, and the mass percentage concentration of the acetic acid is 10-15%.
Further, in the preparation method of the nano hydrated silicon dioxide super-hydrophobic modification, the polyalcohol is formed by compounding polyethylene glycol and ethanol according to the mass ratio of 1: 1-2.
Further, in the method for preparing the nano hydrated silicon dioxide through super-hydrophobic modification, the mass ratio of the hydrolysate to the total feeding amount in the reaction kettle is 2.0-5.0%.
Further, in the above super-hydrophobic modified preparation method of nano hydrated silicon dioxide, the step 2 is specifically: adding the nano hydrated silicon dioxide into a reaction kettle, sealing the reaction kettle, starting stirring and heating simultaneously, and after the addition of the nano hydrated silicon dioxide is finished, increasing the stirring speed to 25-35 r/min to ensure that the nano hydrated silicon dioxide is stirred at a high speed into a fluid state in a sealed reaction vessel.
Further, in the above preparation method for superhydrophobic modification of nano hydrated silica, the step 4 specifically is: after the reaction is finished, opening a pressure release valve of the reaction kettle to release pressure, recovering the desorbed ammonia gas through the absorption tower, closing the pressure release valve, introducing high-pressure nitrogen into the closed reaction kettle to increase the pressure in the reaction kettle again to reach 3-4 MPa, slowly releasing the pressure, and recovering the desorbed ammonia gas through the absorption tower.
Further, in the preparation method for the superhydrophobic modification of the nano hydrated silicon dioxide, the atomization speed is 500-800 mL/min.
Further, in the preparation method of the nano hydrated silicon dioxide super-hydrophobic modification, in the step 1, a silane coupling agent is selected and compounded by hexamethyldisilazane and one or more than two of A-171, A-151 and KH560 according to the mass ratio of 4.5: 1-2.5.
The invention has the beneficial effects that: two silane coupling agents are adopted for hydrolysis, and then the silane coupling agents and the nano hydrated silicon dioxide are subjected to gas-solid reaction under the gasification temperature and the closed condition, the silane coupling agents are hydrolyzed in advance, so that the reaction is quicker and more sufficient, the organic functional groups replace the hydroxyl of the nano water and the silicon dioxide to the maximum extent and are grafted to the nano hydrated silicon dioxide structure, and the modified silicon dioxide is changed from hydrophilicity to lipophilicity, so that the purpose of super hydrophobicity is achieved. The ammonia gas generated as a byproduct in the reaction with the silane coupling agent is difficult to completely remove only by means of pressure relief or vacuum pumping. In the invention, after the modification reaction is finished, firstly, the reaction kettle is decompressed for one time to remove most of ammonia gas, then the decompression valve is closed, nitrogen gas is introduced into the reaction kettle to pressurize the reaction kettle again, in the pressurizing process, as the concentration of the ammonia gas is far lower than that of the nitrogen gas, the nitrogen gas can be used for driving the ammonia gas remained in the pores in the hydrophobic modified nano hydrated silicon dioxide, and the nitrogen gas is used for filling the pores, the pressure is relieved again, and the vacuum pumping is carried out to completely remove the remained ammonia gas, as the nitrogen gas belongs to neutral gas, the pH value of the hydrophobic nano hydrated silicon dioxide can be maintained neutral in the nitrogen environment, so that the prepared super-hydrophobic nano hydrated silicon dioxide can not influence the acid-base balance of the organic phase system of the polysiloxane system, and can not cause the organic phase polymerization or decomposition of the polysiloxane system.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
Example 1
A method for preparing nano hydrated silicon dioxide by super-hydrophobic modification comprises the following steps:
step 1: hydrolysis of a coupling agent: respectively weighing 5kg of hexamethyldisilazane and 2kgA-171, adding hydrolysate which is prepared by compounding 1kg of 15% acetic acid, 2kg of water, 1kg of polyethylene glycol and 1kg of ethanol in advance, and hydrolyzing, wherein the coupling agent hydrolysate needs to be used up within 1 hour;
step 2: adding 100kg of nano hydrated silicon dioxide into a closed reaction kettle, starting stirring and heating simultaneously, and after the addition of the nano hydrated silicon dioxide is finished, increasing the stirring speed to 30 revolutions per minute to ensure that the nano hydrated silicon dioxide is stirred at a high speed into a fluid state in a closed reaction vessel;
and step 3: and (3) after the temperature of the materials in the reaction kettle rises to 100 ℃, spraying the coupling agent hydrolyzed in the step (1) into the reaction kettle in an atomization mode, wherein the spraying speed is 500 mL/min. Heating the materials to 125 deg.C, sealing and reacting for 30min
And 4, step 4: after the reaction is finished, opening a pressure release valve of the reaction kettle to release pressure, recovering the desorbed ammonia gas through the absorption tower, closing the pressure release valve, introducing high-pressure nitrogen into the closed reaction kettle to enable the pressure in the reaction kettle to rise again to reach 3.5MPa, slowly releasing the pressure, and recovering the desorbed ammonia gas through the absorption tower.
And 5: and (3) after the pressure is relieved to normal pressure, carrying out negative pressure air extraction on the reaction kettle for 15min, wherein the negative pressure is-0.02 MPa, and finally obtaining the super-hydrophobic nano hydrated silicon dioxide. Sampling to measure the methanol value and the pH value.
Example 2
A method for preparing nano hydrated silicon dioxide by super-hydrophobic modification comprises the following steps:
step 1: hydrolysis of a coupling agent: respectively weighing 4.5kg of hexamethyldisilazane and 2.5kgA-151, adding hydrolysate which is prepared by compounding 1kg of 12% acetic acid, 2kg of water, 1.2kg of polyethylene glycol and 1.5kg of ethanol in advance, and hydrolyzing, wherein the coupling agent hydrolysate needs to be used up within 1 hour;
step 2: adding 100kg of nano hydrated silicon dioxide into a closed reaction kettle, starting stirring and heating simultaneously, and after the addition of the nano hydrated silicon dioxide is finished, increasing the stirring speed to 30 revolutions per minute to ensure that the nano hydrated silicon dioxide is stirred at a high speed into a fluid state in a closed reaction vessel;
and step 3: after the temperature of the materials in the kettle is raised to 110 ℃,
and (3) spraying the coupling agent hydrolyzed in the step (1) into the reaction kettle in an atomization mode, wherein the spraying speed is 500 mL/min. Heating the materials to 130 deg.C, sealing and reacting for 40min
And 4, step 4: after the reaction is finished, opening a pressure release valve of the reaction kettle to release pressure, recovering the desorbed ammonia gas through the absorption tower, closing the pressure release valve, introducing high-pressure nitrogen into the closed reaction kettle to enable the pressure in the reaction kettle to rise again to reach 3.5MPa, slowly releasing the pressure, and recovering the desorbed ammonia gas through the absorption tower.
And 5: and (3) after the pressure is relieved to normal pressure, carrying out negative pressure air extraction on the reaction kettle for 20min, wherein the negative pressure is-0.02 MPa, and finally obtaining the super-hydrophobic nano hydrated silicon dioxide. Sampling to determine the methanol value and the pH value.
Example 3
A method for preparing nano hydrated silicon dioxide by super-hydrophobic modification comprises the following steps:
step 1: hydrolysis of a coupling agent: respectively weighing 4.5kg of hexamethyldisilazane, 1kgA-151 kg of hexamethyldisilazane and 1kg of KH560, adding hydrolysate prepared by compounding 1kg of 10% acetic acid, 2.5kg of water, 1.5kg of polyethylene glycol and 2kg of ethanol in advance, and hydrolyzing, wherein the coupling agent hydrolysate needs to be used up within 1 hour;
step 2: adding 100kg of nano hydrated silicon dioxide into a closed reaction kettle, starting stirring and heating simultaneously, and after the addition of the nano hydrated silicon dioxide is finished, increasing the stirring speed to 30 revolutions per minute to ensure that the nano hydrated silicon dioxide is stirred at a high speed into a fluid state in a closed reaction vessel;
and step 3: after the temperature of the materials in the kettle is raised to 110 ℃,
and (3) spraying the coupling agent hydrolyzed in the step (1) into the reaction kettle in an atomization mode, wherein the spraying speed is 500 mL/min. Heating the materials to 140 deg.C, sealing and reacting for 45min
And 4, step 4: after the reaction is finished, opening a pressure release valve of the reaction kettle to release pressure, recovering the desorbed ammonia gas through the absorption tower, closing the pressure release valve, introducing high-pressure nitrogen into the closed reaction kettle to enable the pressure in the reaction kettle to rise again to reach 4MPa, slowly releasing the pressure, and recovering the desorbed ammonia gas through the absorption tower.
And 5: and (3) after the pressure is relieved to normal pressure, carrying out negative pressure air extraction on the reaction kettle for 15min, wherein the negative pressure is-0.02 MPa, and finally obtaining the super-hydrophobic nano hydrated silicon dioxide. Sampling to determine the methanol value and the pH value.
Comparative example 1
A preparation method of nano hydrated silica through hydrophobic modification comprises the following steps:
step 1: adding 100kg of nano hydrated silicon dioxide into a closed reaction kettle, starting stirring and heating simultaneously, and after the addition of the nano hydrated silicon dioxide is finished, increasing the stirring speed to 30 revolutions per minute to ensure that the nano hydrated silicon dioxide is stirred at a high speed into a fluid state in a closed reaction vessel;
step 2: after the temperature of the materials in the kettle rises to 100 ℃, 10kg of hexamethyldisilazane and a hydrophobic assistant are sprayed in sequence in an atomization mode, and the spraying atomization speed is 500 mL/min;
heating the material to 130 ℃ and reacting for 40 min; the auxiliary hydrophobic agent is prepared from 15 percent of acetic acid and 97 percent of water, the mass ratio of the auxiliary hydrophobic agent to the total feeding amount in the reaction kettle is 1.5 percent,
and step 3: after the reaction is finished, opening a pressure release valve of the reaction kettle to release pressure, and recovering the desorbed ammonia gas through an absorption tower. And (3) after the pressure is relieved to normal pressure, carrying out negative pressure air extraction on the reaction kettle for 15min, wherein the negative pressure is-0.02 MPa, and finally preparing the hydrophobically modified nano hydrated silicon dioxide. Sampling to measure the methanol value and the pH value.
Comparative example 2
A preparation method of nano hydrated silica through hydrophobic modification comprises the following steps:
step 1: adding 100kg of nano hydrated silicon dioxide into a closed reaction kettle, starting stirring and heating simultaneously, and after the addition of the nano hydrated silicon dioxide is finished, increasing the stirring speed to 30 revolutions per minute to ensure that the nano hydrated silicon dioxide is stirred at a high speed into a fluid state in a closed reaction vessel;
step 2: after the temperature of the materials in the kettle rises to 110 ℃, 12kg of hexamethyldisilazane and a hydrophobic assistant are sprayed in sequence in an atomization mode, and the spraying atomization speed is 500 mL/min;
heating the material to 135 ℃ and reacting for 50 min; the auxiliary hydrophobic agent is prepared from 10 percent of acetic acid and 97 percent of water, the mass ratio of the auxiliary hydrophobic agent to the total feeding amount in the reaction kettle is 1.5 percent,
and step 3: after the reaction is finished, opening a pressure release valve of the reaction kettle to release pressure, and recovering the desorbed ammonia gas through an absorption tower. And (3) after the pressure is relieved to normal pressure, carrying out negative pressure air extraction on the reaction kettle for 15min, wherein the negative pressure is-0.02 MPa, and finally preparing the hydrophobically modified nano hydrated silicon dioxide. Sampling to measure the methanol value and the pH value.
Table 1 shows the measured methanol values and pH values of the hydrophobic nano hydrated silicas obtained in examples 1 to 3 and comparative examples 1 to 2.
TABLE 1
As shown in Table 1, the super-hydrophobic product with methanol value of more than 70 can be prepared by the preparation method of compounding two or more specific silane coupling agents and carrying out composite treatment on the nano hydrated silicon dioxide in a pre-hydrolysis mode, and the final pH value of the product is less than 7.5. In comparative examples 1-2, the methanol value of the hydrophobically modified nano hydrated silica powder was measured to be about 60 and the pH value was measured to be greater than 8 without the secondary pressurization and depressurization process by adding nitrogen, which indicates that the trial-produced product has a general hydrophobic effect and the residual ammonia gas is not completely removed.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (8)
1. A method for preparing nano hydrated silicon dioxide by super-hydrophobic modification is characterized by comprising the following steps:
step 1: adding hydrolysate prepared by compounding organic acid, water and polyalcohol into silane coupling agent for hydrolysis, wherein the silane coupling agent is prepared by compounding hexamethyldisilazane and one or more than two of A-171, A-151 or KH 560;
Step 2: adding the nano hydrated silicon dioxide into a reaction kettle, sealing the reaction kettle, starting stirring and heating;
and step 3: after the temperature of the material is raised to 100-110 ℃, spraying the hydrolyzed coupling agent solution into a reaction kettle in a fogging manner, raising the temperature of the material to 120-140 ℃, and carrying out a closed reaction for 30-50 min;
and 4, step 4: after the reaction is finished, opening a pressure release valve of the reaction kettle for pressure release, and then closing the pressure release valve; introducing high-pressure nitrogen into the closed reaction kettle, raising the pressure in the reaction kettle again to 3-4 MPa, maintaining for 30-50 min, and then slowly releasing the pressure;
and 5: and (3) after the pressure is relieved to normal pressure, performing negative pressure air extraction on the reaction kettle for 10-20 min, wherein the negative pressure is-0.03 MPa to-0.01 MPa, and finally preparing the super-hydrophobic modified nano hydrated silicon dioxide product.
2. The method for preparing the nano hydrated silica through super hydrophobic modification according to claim 1, wherein the organic acid is selected from acetic acid, and the concentration of the acetic acid in percentage by mass is 10-15%.
3. The method for preparing the nano hydrated silicon dioxide through superhydrophobic modification according to claim 1, wherein the polyalcohol is formed by compounding polyethylene glycol and ethanol according to a mass ratio of 1: 1-2.
4. The method for preparing the nano hydrated silica through super-hydrophobic modification according to claim 1, wherein the hydrolysis liquid accounts for 2.0-5.0% of the total feeding amount in the reaction kettle by mass ratio.
5. The method for preparing nano hydrated silica through superhydrophobic modification according to claim 1, wherein the step 2 specifically comprises: adding the nano hydrated silicon dioxide into a reaction kettle, sealing the reaction kettle, starting stirring and heating simultaneously, and after the addition of the nano hydrated silicon dioxide is finished, increasing the stirring speed to 25-35 r/min to ensure that the nano hydrated silicon dioxide is stirred at a high speed into a fluid state in a sealed reaction vessel.
6. The method for preparing nano hydrated silica through superhydrophobic modification according to claim 1, wherein the step 4 specifically comprises: after the reaction is finished, opening a pressure release valve of the reaction kettle to release pressure, recovering the desorbed ammonia gas through the absorption tower, closing the pressure release valve, introducing high-pressure nitrogen into the closed reaction kettle to increase the pressure in the reaction kettle again to reach 3-4 MPa, slowly releasing the pressure, and recovering the desorbed ammonia gas through the absorption tower.
7. The method for preparing the nano hydrated silica through superhydrophobic modification according to claim 1, wherein the atomization speed is 500-800 mL/min.
8. The hydrophobic nano hydrated silicon dioxide prepared by the super-hydrophobic modification preparation method of nano hydrated silicon dioxide as claimed in any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210365109.XA CN114836057B (en) | 2022-04-07 | 2022-04-07 | Preparation method of nano hydrated silicon dioxide through superhydrophobic modification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210365109.XA CN114836057B (en) | 2022-04-07 | 2022-04-07 | Preparation method of nano hydrated silicon dioxide through superhydrophobic modification |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114836057A true CN114836057A (en) | 2022-08-02 |
| CN114836057B CN114836057B (en) | 2023-06-09 |
Family
ID=82563712
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210365109.XA Active CN114836057B (en) | 2022-04-07 | 2022-04-07 | Preparation method of nano hydrated silicon dioxide through superhydrophobic modification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114836057B (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3924029A (en) * | 1962-03-30 | 1975-12-02 | Degussa | Method of modifying the surface properties of finely divided metal oxides |
| US4715986A (en) * | 1984-03-30 | 1987-12-29 | Th. Goldschmidt Ag | Particles, modified at their surface by hydrophilic and hydrophobic groups |
| US5919298A (en) * | 1998-01-12 | 1999-07-06 | Dow Corning Corporation | Method for preparing hydrophobic fumed silica |
| JP2001281914A (en) * | 2000-03-31 | 2001-10-10 | Nippon Aerosil Co Ltd | Surface-modified metal oxide fine powder and its production method and use |
| CN102220036A (en) * | 2011-06-02 | 2011-10-19 | 北京化工大学 | Method for preparing white carbon black modified by silane coupling agent |
| DE102011120843A1 (en) * | 2011-12-13 | 2013-06-13 | Bayerisches Zentrum für Angewandte Energieforschung e.V. | Sol-gel process to produce porous, hydrophobic silica-containing xerogel, where the hydrophobicity is produced in situ during the process and alkoxysilane e.g. tetramethoxysilane is used as the silica source, useful e.g. as filler |
| CN103992701A (en) * | 2014-05-23 | 2014-08-20 | 中国人民武装警察部队杭州士官学校 | Method for preparing super hydrophobic polymer composite coating containing nano particles and product thereof |
| CN105733423A (en) * | 2016-03-14 | 2016-07-06 | 江苏中涂涂料检测中心有限公司 | Silane coupling agent hydrolysate and application thereof in polyaniline attapulgite nano composite coating |
| CN107973935A (en) * | 2017-12-07 | 2018-05-01 | 沈阳化工大学 | A kind of modified white carbon black and preparation method thereof |
| CN108441026A (en) * | 2018-04-25 | 2018-08-24 | 福建远翔新材料股份有限公司 | A kind of dewatering nano hydrated SiO 2 and its preparation method and application |
| CN111655802A (en) * | 2018-01-25 | 2020-09-11 | 卡博特公司 | Aqueous hydrophobic silica dispersion |
| CN113150387A (en) * | 2021-04-21 | 2021-07-23 | 江苏联瑞新材料股份有限公司 | Preparation method of hydrophobic silicon micro powder |
-
2022
- 2022-04-07 CN CN202210365109.XA patent/CN114836057B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3924029A (en) * | 1962-03-30 | 1975-12-02 | Degussa | Method of modifying the surface properties of finely divided metal oxides |
| US4715986A (en) * | 1984-03-30 | 1987-12-29 | Th. Goldschmidt Ag | Particles, modified at their surface by hydrophilic and hydrophobic groups |
| US5919298A (en) * | 1998-01-12 | 1999-07-06 | Dow Corning Corporation | Method for preparing hydrophobic fumed silica |
| JP2001281914A (en) * | 2000-03-31 | 2001-10-10 | Nippon Aerosil Co Ltd | Surface-modified metal oxide fine powder and its production method and use |
| CN102220036A (en) * | 2011-06-02 | 2011-10-19 | 北京化工大学 | Method for preparing white carbon black modified by silane coupling agent |
| DE102011120843A1 (en) * | 2011-12-13 | 2013-06-13 | Bayerisches Zentrum für Angewandte Energieforschung e.V. | Sol-gel process to produce porous, hydrophobic silica-containing xerogel, where the hydrophobicity is produced in situ during the process and alkoxysilane e.g. tetramethoxysilane is used as the silica source, useful e.g. as filler |
| CN103992701A (en) * | 2014-05-23 | 2014-08-20 | 中国人民武装警察部队杭州士官学校 | Method for preparing super hydrophobic polymer composite coating containing nano particles and product thereof |
| CN105733423A (en) * | 2016-03-14 | 2016-07-06 | 江苏中涂涂料检测中心有限公司 | Silane coupling agent hydrolysate and application thereof in polyaniline attapulgite nano composite coating |
| CN107973935A (en) * | 2017-12-07 | 2018-05-01 | 沈阳化工大学 | A kind of modified white carbon black and preparation method thereof |
| CN111655802A (en) * | 2018-01-25 | 2020-09-11 | 卡博特公司 | Aqueous hydrophobic silica dispersion |
| CN108441026A (en) * | 2018-04-25 | 2018-08-24 | 福建远翔新材料股份有限公司 | A kind of dewatering nano hydrated SiO 2 and its preparation method and application |
| CN113150387A (en) * | 2021-04-21 | 2021-07-23 | 江苏联瑞新材料股份有限公司 | Preparation method of hydrophobic silicon micro powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114836057B (en) | 2023-06-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2017185874A1 (en) | Hydroxyl silicone oil and continuous method for preparing same | |
| CN112694717B (en) | Preparation method of mixed hollow glass bead solid buoyancy material | |
| CN104479363A (en) | Low-compression-deformation two-component addition-type low-hardness silicon rubber and preparation method thereof | |
| CN106700545B (en) | A kind of compound abrasive rubber material | |
| CN115368806B (en) | Anticorrosive paint applied to petroleum pipeline and preparation method thereof | |
| CN107201170A (en) | A kind of silicone sealant containing microcapsules and preparation method thereof | |
| CN109180941B (en) | A kind of preparation method of organic-inorganic hybrid octafunctional epoxy POSS resin and preparation method of carbon fiber reinforced composite material | |
| CN114836057B (en) | Preparation method of nano hydrated silicon dioxide through superhydrophobic modification | |
| CN113604193A (en) | Organosilicon sealant and preparation method thereof | |
| CN114349485B (en) | Preparation method of high-hardness alumina ceramic | |
| CN109971047B (en) | Natural rubber-white carbon black composite material and preparation method and application thereof | |
| CN115466488A (en) | A kind of hollow spherical silica epoxy resin composite material and its preparation method and application | |
| CN114790342A (en) | Silane modified carbon black composite filler and preparation method thereof | |
| CN113980426A (en) | A kind of modified graphene toughened epoxy resin heat-resistant composite material and preparation method thereof | |
| CN103897195A (en) | Method for preparing alkoxy terminated polydimethylsiloxane | |
| CN108441026A (en) | A kind of dewatering nano hydrated SiO 2 and its preparation method and application | |
| CN109852338A (en) | Fluorosilicone rubber composition, preparation method and the sealant and coating prepared by the composition | |
| CN111099876A (en) | A kind of preparation method of low-cost silica aerogel composite flexible thermal insulation material | |
| CN106590052A (en) | Polydopamine polyethenoxy ether active agent modified shape-controllable nano calcium carbonate powder and preparation method thereof | |
| CN111704817A (en) | Water-resistant breathable water-based inorganic coating and preparation method thereof | |
| CN115124876B (en) | Functional filler, water-based anti-icing paint for wind power blade and preparation method of anti-icing paint | |
| CN113957721B (en) | Anti-wrinkle elastic silicone oil and preparation method thereof | |
| CN115851217A (en) | Single-component room temperature vulcanized silicone pouring sealant for display screen and preparation method thereof | |
| CN109852071A (en) | Fluorosilicone rubber composition, preparation method and the sealant and coating prepared by the composition | |
| CN107236482B (en) | A kind of multi-arm LED packaging plastic strengthening helping agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |